Analysis of thyreostatic drugs in thyroid samples by Ultra-Performance Liquid Chromatography tandem mass spectrometry detection

作者：Abuinb S; Centrich F; Rubies A; Companyo R^*; Prat M D

来源：Analytica Chimica Acta, 2008, 617(1-2): 184-191.

DOI：10.1016/j.aca.2007.12.018

• thyreostatic drugs
• thyroid samples
• ultra-performance liquid chromatography
• liquid chromatography tandem mass spectrometry detection

A method based on ultra-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry for the determination of six thyreostatic drugs in thyroid tissue has been optimised and validated in accordance with the Decision 2002/657/EC. Samples are extracted with methanol and the extracts cleaned-up on silica cartridges. The recoveries range from 40% for 6-phenyl-2-thiouracil to 79% for 2-thiouracil. Quantification is carried out with blank tissue samples spiked with the analytes in the range 25-500 mu g kg(-1). 5,6-Dimethyl-2-thiouracil is used as internal standard. CC alpha and CC beta are in the ranges 4.3-16.1 mu g kg(-1) and 8.7-20.7 mu g kg(-1), respectively. Accuracy, expressed as percentage of error, is lower than 6% and relative standard deviation in reproducibility conditions falls between 5.6 and 10.3%. Nowadays, the proposed method is routinely implemented in the laboratory of the Agencia de Salut Publica de Barcelona and allows processing of up to 20 samples per day.

• 出版日期2008-6-9